CN110980900A - Modified powder zeolite-loaded Fe3O4Coupling compound coagulant aid, preparation method and application - Google Patents
Modified powder zeolite-loaded Fe3O4Coupling compound coagulant aid, preparation method and application Download PDFInfo
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- CN110980900A CN110980900A CN201911274902.3A CN201911274902A CN110980900A CN 110980900 A CN110980900 A CN 110980900A CN 201911274902 A CN201911274902 A CN 201911274902A CN 110980900 A CN110980900 A CN 110980900A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
Abstract
The invention discloses modified powder zeolite-loaded Fe3O4Coupling compound coagulant aid, preparation method and application, natural zeolite powder modification A; preparing suspension by using modified zeolite powder A to prepare the supported nascent state Fe3O4Modified zeolite powder B; preparing ferric trichloride and Na2SiO 3.9H 2O solution to form a composite coagulant aid, adding 1-5 mg/L of the composite coagulant aid in a rapid reaction stage after adding the coagulant aid, and adding 0.1-1.0 mg/L of load nascent state Fe in the initial flocculation stage3O4Modified zeolite powder B. The method has the advantages of simple operation, cheap and easily obtained materials, no introduction of toxic and harmful pollutants and high safety; can strengthen the treatment effect of low-temperature low-turbidity high ammonia nitrogen water, and the modified material can be regenerated and reused. The method has the advantages of high efficiency, safety, economy, greenness and the like, and has important meaning for the application of the low-temperature low-turbidity high-ammonia nitrogen water quality reinforced coagulation treatment technologyLeading significance.
Description
Technical Field
The invention relates to a water treatment technology, in particular to a modified powder zeolite-loaded Fe3O4A coupling compound coagulant aid, a preparation method and application.
Background
The low-temperature low-turbidity water has the characteristics of large viscosity, small quantity of colloid impurities, small particle size of impurity particles and the like. Because the water temperature is lower, the zeta potential absolute value of the particles is higher, the repulsion force between the particles is larger, the particles are not easy to destabilize in the coagulation process, and the generated flocs have small particle size, low density and poorer precipitation and filtration effects; meanwhile, the number of particles in water is small, so that the effective collision times and frequency among the particles are small, and the flocculation reaction process is influenced. After the water preparation is finished, small particulate matters in the water easily continue to exist in the water and are difficult to remove. The turbidity of the drinking water and the Ames mutation ratio show positive correlation, and the health risk is higher if the turbidity of the drinking water is large. At present, a high-efficiency, safe and economic coagulant aid is needed to enhance coagulation and improve the low-temperature and low-turbidity water treatment effect.
Ammonia nitrogen pollution generally exists in drinking surface water in China, and can provide nutrition for algae in water, so that the algae are massively propagated, and the water quality safety is influenced; in the process of the water production process, the water production cost, the consumption of chlorine and the generation amount of disinfection byproducts are increased, and in the process of pipe network water transmission and distribution, the propagation of pipeline bacteria is promoted to cause water quality pollution. High-concentration ammonia nitrogen enters a human body through drinking water, diet and other ways, nitrite nitrogen and nitrate nitrogen substances are generated in the conversion process of the ammonia nitrogen, and diseases such as methemoglobinemia, gastric cancer, liver cancer and the like can be caused, so that sufficient attention and attention should be paid to ammonia nitrogen pollution of a water body. The conventional treatment process is reinforced by pre-adsorption, so that the removal effect of pollutants can be economically and efficiently improved. Zeolite is a cheap, easily available and safe natural mineral, is used as a common adsorbent material, and can remove ammonia nitrogen by utilizing the ion exchange characteristic of the zeolite. However, the adsorption of the natural zeolite on ammonia nitrogen is far from the theoretical adsorption capacity due to surface impurities and blockage of internal pore channels, and meanwhile, the zeolite powder adsorbent with small particle size can increase the turbidity of effluent to a certain extent in the water purification process.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to solve the defect of removing ammonia nitrogen in micro-polluted water by natural zeolite powder and provide a modified powder zeolite-loaded Fe3O4A coupling compound coagulant aid, a preparation method and application.
The invention solves the technical problems by the following technical scheme, and discloses modified powder zeolite-loaded Fe3O4The preparation method of the coupling compound coagulant aid comprises the following steps:
(1) taking natural zeolite powder, cleaning, removing impurities and drying for later use;
(2) carrying out acid-salt-high temperature modification on natural zeolite powder, grinding and sieving to obtain modified zeolite powder A;
(3) mixing ferrous chloride and ferric trichloride solution, quickly stirring to form a solution A, slowly dropwise adding ammonia water with the volume of 10-15 times of the solution A, performing magnetic separation, removing supernatant, repeatedly washing to neutrality, adding water, performing ultrasonic sealing, and storing to obtain nascent state Fe3O4A suspension of particles;
(4) mixing Fe3O4Mixing the particle suspension and the modified zeolite powder suspension A, stirring and precipitating, cleaning the precipitate, drying and grinding to obtain the supported nascent state Fe3O4Modified zeolite powder;
(5) mixing Na2SiO3·9H2Slowly dripping the O solution into ferric trichloride to prepare a Fe/Si composite coagulant aid with the mass ratio of 1: 1-2, wherein the stabilization period is 10-20 days;
in a preferred embodiment of the present invention, in the step (1), the natural zeolite powder is off-white, has a particle size of 50 to 200 mesh, contains at least 93% of silicon, aluminum, and oxygen in total, and contains a small amount of potassium, calcium, sodium, magnesium, iron, and the like.
In a preferred embodiment of the present invention, in the step (2), the natural zeolite powder is stirred and immersed in 0.05 to 0.1mol/L hydrochloric acid solution for 2 to 4 hours, and then washed to be neutral; after drying and grinding, taking a proper amount of sample, stirring and dipping the sample in 0.8-1.2 mol/L sodium chloride solution for 20-24 h, and washing to remove residual sodium chloride; roasting at 450-500 ℃ for 2-3 h, grinding and sieving to obtain 100-200 mesh modified zeolite powder A.
As one preferable mode of the invention, in the step (3), 2mol/L ferrous chloride and 1mol/L ferric trichloride solution in a volume ratio of 1:4 are mixed and then rapidly stirred to form a solution A, 1mol/L ammonia water with the volume 10-15 times that of the solution A is slowly dripped, a magnet is placed at the bottom of a container, a supernatant is discarded, the magnet is removed and repeatedly washed to be neutral, high-purity water with the volume 1-5 times that of the solution A is added, the mixture is subjected to ultrasonic treatment for 5-10 min and then is sealed for storage, and the nascent state Fe is prepared3O4A suspension of particles.
In a preferred embodiment of the present invention, in the step (4), the modified zeolite powder a is disposed in a modified zeolite powder suspension a, and Fe is added3O4Mixing the particle suspension and the modified zeolite powder suspension A according to a mass ratio of 1: 1-2, mechanically stirring for 4-8 h, cleaning precipitates after static precipitation, drying and grinding to obtain 100-200-mesh supported nascent state Fe3O4Modified zeolite powder.
In a preferred embodiment of the present invention, in the step (5), Na is added2SiO3·9H2And slowly dripping the O solution into ferric trichloride, quickly stirring in the reaction process, ensuring that no floc is deposited in the whole process, forming a reddish brown solution to form a composite coagulant aid with the Fe/Si ratio of 1: 1-2, and stabilizing for 10-20 days.
The invention also discloses a compound coagulant aid prepared by the preparation method.
As one of the preferable modes of the invention, 1-5 mg/L of compound coagulant aid is added in the rapid reaction stage of the coagulation process of water treatment.
As one of the preferable modes of the invention, 0.1-1.0 mg/L of the novel ecological Fe3O 4-loaded modified zeolite powder is added at the initial flocculation stage of the coagulation process of water treatment;
as one of the preferable modes of the invention, the modified zeolite powder after water treatment is subjected to solid-liquid separation by using a magnetic separation technology, and the recovered modified zeolite powder is washed clean, then is put into a sodium chloride solution of 0.8-2.0 mol/L, is stirred, soaked, cleaned, dried, ground and sieved to obtain the zeolite powder.
The natural zeolite modification process is as follows: after acid-salt-high temperature modification, the specific surface area of the zeolite powder is increased, impurities in holes and channels are removed, the holes are dredged, restored and reconstructed, the porosity and the pore volume are increased, and the adsorption rate and the cation exchange capacity are improved, so that the exchange adsorption capacity of the zeolite to ammonia nitrogen is enhanced.
The compounded coagulant aid enables the micro-flocs to be mutually bonded and easier to aggregate and combine, and flocs with larger specific surface area and structure are formed. The floc morphology changes because the result of different actions has been produced to colloidal particle and suspended solid granule in aqueous, and the electric property is in the coagulation machine and the effort of compressing the two electron layers is strong and weak different, and the floc morphology structure that forms is also different, and the existence of compound coagulant aid makes colloid and suspended particles in aqueous still have adsorption bridge and the sweeping precipitation effect of book to the floc of formation is thick closely knit, easily subsides.
Compared with the prior art, the invention has the following advantages: the invention selects a proper zeolite powder modification method, couples the modified zeolite powder with the compound coagulant aid to strengthen the low-temperature low-turbidity high-ammonia nitrogen water treatment, and simultaneously utilizes the magnetic separation technology to quickly recover the modified zeolite powder and regenerate for reuse. The method has the advantages of simple operation, cheap and easily obtained materials, no introduction of toxic and harmful pollutants and high safety; can strengthen the treatment effect of low-temperature low-turbidity high ammonia nitrogen water. The method has the advantages of safety, high efficiency, economy and environmental friendliness, and has important guiding significance for treating micro-polluted low-temperature low-turbidity high-ammonia nitrogen water.
Drawings
FIG. 1 is a graph comparing the effect of the coagulant aid prepared according to the present invention on water treatment;
FIG. 2 is a comparison of the topography of coagulation aid alone and using the present invention.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The specific preparation method of this example is as follows:
(1) the natural zeolite powder produced from eastern town of Jinyun county in Lishui City is selected, the color is grey white, the particle size range is 50-200 meshes, and the content of silicon, aluminum and oxygen is more than 93 percent and contains a small amount of potassium, calcium, sodium, magnesium, iron and other components. And (2) repeatedly cleaning 250g of natural zeolite powder to remove soluble impurities on the surface of the zeolite powder, fully stirring and soaking for at least 2h in the cleaning process to reduce the alkalinity of the zeolite powder, and then drying the zeolite powder in an oven at 110 ℃ for later use.
(2) Taking a proper amount of the natural zeolite powder obtained in the step (1), stirring and soaking in 0.1mol/L hydrochloric acid solution for 2 hours, and then cleaning to be neutral; drying and grinding the sample in a drying oven at 90 ℃, then taking 150g of the sample, stirring and soaking the sample in 1.0mol/L sodium chloride solution for 24 hours, and washing the sample for multiple times to remove residual sodium chloride; placing the mixture in a muffle furnace, raising the temperature to 450 ℃, roasting for 2h, grinding and sieving to obtain the 200-mesh modified zeolite powder A.
(3) 1ml of 2mol/L FeCl is taken2And 4ml of 1mol/L ferric chloride are placed in a small beaker to be fully stirred, 50ml of 1mol/L ammonia water is used for slowly titrating, the titration is slower, the titration is finished within 5min, after the reaction is finished, a magnet is placed at the bottom of the beaker, supernatant is poured out, the magnet is removed and repeatedly washed, and finally 5ml of water is taken and added with the nascent state Fe3O4In the granules, performing ultrasonic treatment for 5min, and sealing and storing to obtain nascent state Fe3O4A suspension of particles.
(4) Preparing modified zeolite powder A with a certain mass into modified zeolite powder suspension A, and adding Fe3O4Mixing the particle suspension and the modified zeolite powder A suspension according to the mass ratio of 1:1, and mechanically stirring for 8 hours. Cleaning the precipitate after static precipitation, drying and grinding the precipitate in an oven at 45 ℃, and preparing the nascent state Fe with the load of 100-200 meshes through a standard sieve3O4Modified zeolite powder.
(5) 10mg/L ferric trichloride calculated by Fe and 10mg/L Na calculated by Si2SiO3·9H2O solution, wherein the pH of ferric trichloride<3; 50ml of Na are taken2SiO3·9H2The O solution is slowly dripped into ferric trichloride to be compounded into a composite coagulant aid with Fe/Si of 1/1, the mixture is rapidly stirred in the reaction process, no floc deposition is ensured in the whole process, the solution is reddish brown, and the mixture can be stably stored for 20 days after being prepared.
(6) After the coagulant is added, 3mg/L of compound coagulant aid is added in the fast reaction stage of the coagulation process.
(7) Adding 0.35mg/L load nascent state Fe at the initial flocculation stage in the coagulation process3O4Modified zeolite powder.
(8) And (2) rapidly performing solid-liquid separation on the modified zeolite powder after water treatment by using a magnetic separation technology, washing the recovered modified zeolite powder, putting the washed modified zeolite powder into 1.2mol/L sodium chloride solution, stirring and soaking for 24 hours, washing, putting the washed modified zeolite powder into an oven, drying at 50 ℃, grinding and sieving to obtain 100-200-mesh zeolite powder, and repeatedly using for more than 2 times.
Example 2
In the embodiment, 0mg/L, 1mg/L, 2mg/L, 4mg/L and 5mg/L compound coagulant aids are respectively added in the fast reaction stage of the coagulation process. Other embodiments are the same as example 1.
Example 3
In the embodiment, the neoecological Fe load is respectively added at the initial flocculation stage of the coagulation process by 0mg/L, 0.2mg/L, 0.55mg/L, 0.8mg/L and 1mg/L3O4Modified zeolite powder. Other embodiments are the same as example 1.
Example 4
In the embodiment, 0mg/L, 0.2mg/L, 0.35mg/L, 0.55mg/L, 0.8mg/L and 1mg/L of common zeolite powder are respectively added at the initial flocculation stage in the coagulation process. Other embodiments are the same as example 1.
As shown in figure 1, the modified powder zeolite-loaded nascent state Fe3O4 coupled compound coagulant aid can obviously improve the treatment effect of low-temperature low-turbidity high-ammonia nitrogen water. The left graph shows the effect of the compound coagulant aid on removing turbidity and TOC of low-temperature low-turbidity high-ammonia nitrogen water after being added, and the removal rate is increased along with the increase of the adding amount, but the removal effect tends to be stable after reaching 3 mg/L.
The right picture is the comparison of the adding effect of the natural zeolite powder and the modified zeolite powder, and it can be seen that the effect of the modified zeolite powder on removing ammonia nitrogen is obviously higher than that of the unmodified natural zeolite powder.
As shown in FIG. 2, the flocs formed by the single coagulation are relatively flat, smooth and flaky; the appearance of floc formed in the coagulation process of the compound coagulant aid is obviously changed, the surface is rough, uneven and relatively dense, and the floc after coagulation aid-coagulation is obviously increased.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. Modified powder zeolite-loaded Fe3O4The preparation method of the coupling compound coagulant aid is characterized by comprising the following steps:
(1) taking natural zeolite powder, cleaning, removing impurities and drying for later use;
(2) carrying out acid-salt-high temperature modification on natural zeolite powder, grinding and sieving to obtain modified zeolite powder A;
(3) mixing ferrous chloride and ferric trichloride solution, quickly stirring to form a solution A, slowly dropwise adding ammonia water with the volume of 10-15 times of the solution A, performing magnetic separation, removing supernatant, repeatedly washing to neutrality, adding water, performing ultrasonic sealing, and storing to obtain nascent state Fe3O4A suspension of particles;
(4) mixing Fe3O4Mixing the particle suspension and the modified zeolite powder suspension A, stirring and precipitating, cleaning the precipitate, drying and grinding to obtain the supported nascent state Fe3O4Modified zeolite powder;
(5) mixing Na2SiO3·9H2And slowly dripping the O solution into ferric trichloride to prepare the Fe/Si composite coagulant aid with the mass ratio of 1: 1-2, wherein the stabilization period is 10-20 days.
2. The modified powdered zeolite negative of claim 1Carrying Fe3O4The preparation method of the coupling compound coagulant aid is characterized in that in the step (1), the natural zeolite powder is grey white, the particle size range is 50-200 meshes, the total content of silicon, aluminum and oxygen is more than 93%, and the coupling compound coagulant aid contains a small amount of potassium, calcium, sodium, magnesium, iron and other components.
3. The modified powdered zeolite supported Fe of claim 13O4The preparation method of the coupling compound coagulant aid is characterized in that in the step (2), the natural zeolite powder is stirred and soaked in 0.05-0.1 mol/L hydrochloric acid solution for 2-4 hours and then is washed to be neutral; after drying and grinding, taking a proper amount of sample, stirring and dipping the sample in 0.8-1.2 mol/L sodium chloride solution for 20-24 h, and washing to remove residual sodium chloride; roasting at 450-500 ℃ for 2-3 h, grinding and sieving to obtain 100-200 mesh modified zeolite powder A.
4. The modified powdered zeolite supported Fe of claim 13O4The preparation method of the coupling compound coagulant aid is characterized in that in the step (3), 2mol/L ferrous chloride and 1mol/L ferric trichloride solution in a volume ratio of 1:4 are mixed and then rapidly stirred to form a solution A, 1mol/L ammonia water in an amount which is 10-15 times of the volume of the solution A is slowly dripped, a magnet is slowly dripped at the bottom of a container, the supernatant is discarded, the magnet is removed and repeatedly washed to be neutral, high-purity water in an amount which is 1-5 times of the volume of the solution A is added, the mixture is subjected to ultrasonic treatment for 5-10 min and then is sealed for storage, and the nascent state Fe is prepared3O4A suspension of particles.
5. The modified powdered zeolite supported Fe of claim 13O4The preparation method of the coupling compound coagulant aid is characterized in that in the step (4), the modified zeolite powder A is prepared into modified zeolite powder suspension A, and Fe is added3O4Mixing the particle suspension and the modified zeolite powder suspension A according to a mass ratio of 1: 1-2, mechanically stirring for 4-8 h, cleaning precipitates after static precipitation, drying and grinding to obtain 100-200-mesh supported nascent state Fe3O4Modified zeolite powder.
6. The modified powdered zeolite supported Fe of claim 13O4The preparation method of the coupling compound coagulant aid is characterized in that in the step (5), Na is added2SiO3·9H2And slowly dripping the O solution into ferric trichloride, quickly stirring in the reaction process, ensuring that no floc is deposited in the whole process, forming a reddish brown solution to form a composite coagulant aid with the Fe/Si ratio of 1: 1-2, and stabilizing for 10-20 days.
7. The compound coagulant aid prepared by the preparation method according to any one of claims 1 to 6.
8. The method for treating the low-temperature low-turbidity high-ammonia nitrogen water by using the compound coagulant aid of claim 7 is characterized in that 1-5 mg/L of the compound coagulant aid is added in a rapid reaction stage of a coagulation process of water treatment.
9. The method for treating low-temperature low-turbidity high-ammonia nitrogen water according to claim 8, wherein 0.1-1.0 mg/L of the nascent state Fe3O 4-loaded modified zeolite powder is added at the initial flocculation stage of the coagulation process of water treatment.
10. The method for treating low-temperature low-turbidity high-ammonia nitrogen water according to claim 9, wherein the zeolite powder is prepared by performing solid-liquid separation on the modified zeolite powder after water treatment by using a magnetic separation technology, washing the recovered modified zeolite powder, putting the washed modified zeolite powder into 0.8-2.0 mol/L sodium chloride solution, stirring, soaking, cleaning, drying, grinding and sieving.
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| CN112062384A (en) * | 2020-09-24 | 2020-12-11 | 北京工业大学 | Magnetic zeolite coupling magnetic coagulation process |
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